Phase composition and components of mixed Fe(III)–Al(III) hydroxides and oxides obtained by ageing the hydroxides are examined mainly by Mössbauer spectroscopy over a wide range of the Al/Fe atomic ratio. The α‐(Fe1–cAlc)2O3 type oxide and the orthorhombic Al2O3, boehmite, are identified in the system studied. An analysis of Heff as a function of c indicates that the maximum value of c ranges from 0.31 to 0.33 regardless of the mixed oxide preparation method. An analysis of the recoil‐free fraction f′(T) and a subsequent calculation of the force constants of the iron–oxygen bonds show that an increase in “c” leads to their weakening.
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